CN103030768B - Polyurethane acrylate prepolymer and preparation method thereof as well as paint prepared by same - Google Patents

Polyurethane acrylate prepolymer and preparation method thereof as well as paint prepared by same Download PDF

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Publication number
CN103030768B
CN103030768B CN201310004982.7A CN201310004982A CN103030768B CN 103030768 B CN103030768 B CN 103030768B CN 201310004982 A CN201310004982 A CN 201310004982A CN 103030768 B CN103030768 B CN 103030768B
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polyurethane acrylate
acrylate prepolymer
prepolymer
product
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CN103030768A (en
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孙伟圣
王艳伟
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JIUSHENG FLOOR CO Ltd
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JIUSHENG FLOOR CO Ltd
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Abstract

The invention discloses a polyurethane acrylate prepolymer and a preparation method thereof, as well as paint prepared by the polyurethane acrylate prepolymer. The prepolymer comprises the following components in part by mass: 900-1100 parts of hexamethylene diisocyanate, 2-5 parts of dibutyl tin laurate, 400-600 parts of polyethylene glycol, 1-3 parts of hydroquinone and 1000-1300 parts of hydroxyethyl acrylate. According to the invention, the paint prepared by the polyurethane acrylate prepolymer is high in curing rate, can effectively improve gloss, flexibility and adhesion level of floorboards, and is excellent in use effect.

Description

A kind of polyurethane acrylate prepolymer and preparation method thereof and the paint obtained with it
Technical field
The present invention relates to a kind of polyurethane acrylate prepolymer and preparation method thereof, and with paint prepared by this polyurethane acrylate prepolymer, belong to the field of coating of timber floor.
Background technology
Timber floor, with advantages such as abundant gentle, the beautiful texture natures of its natural environmental-protective, texture, enters into average family just more and more.Along with people are for the continuous pursuit of quality of life, the performance requriements of timber floor is also more and more higher.And the paint being coated on wood floor surface plays vital effect for the performance of timber floor, such as polyurethane prepolymer has relatively high toughness, flexibility, solidity to corrosion and adhesion strength, in order to make timber floor have identical feature, start more and more polyurethane prepolymer to be applied to Floor Industry as paint raw materials.But, due to existing polyurethane prepolymer preparation technology and polyurethane prepolymer to be made the preparation technology of corresponding paint more unreasonable, make the solidification rate of the paint obtained lower, and cause the performances such as the glossiness of the timber floor by this paint application, elasticity, snappiness and sticking power grade more undesirable, and the difficult quality of timber floor is finally made to obtain breakthrough.Therefore, how to improve the preparation method of polyurethane prepolymer, and how to improve preparation method polyurethane prepolymer being made paint, become the problem that this area is urgently to be resolved hurrily.
Summary of the invention
Technical problem to be solved by this invention is the paint providing a kind of polyurethane acrylate prepolymer and preparation method thereof and obtain with it.The paint curing speed obtained with this polyurethane acrylate prepolymer is high, and effectively can improve the glossiness on floor, elasticity, snappiness and sticking power grade, and result of use is very superior.
For solving the problems of the technologies described above, technical scheme of the present invention: a kind of polyurethane acrylate prepolymer, this prepolymer comprises hexamethylene diisocyanate 900-1100 part, dibutyl tin laurate 2-5 part, poly(oxyethylene glycol) 400-600 parts, Resorcinol 1-3 part and Hydroxyethyl acrylate 1000-1300 part by mass parts.
In above-mentioned polyurethane acrylate prepolymer, this prepolymer comprises hexamethylene diisocyanate 1000 parts, dibutyl tin laurate 3 parts, polyoxyethylene glycol 500 parts, Resorcinol 2 parts and Hydroxyethyl acrylate 1150 parts by mass parts.
The preparation method of aforesaid polyurethane acrylate prepolymer, the method comprises the following steps;
A, hexamethylene diisocyanate to be mixed with dibutyl tin laurate, and reconcile pH value to 5, then pass into dry nitrogen 5 ~ 10min, stir, obtain A product;
B, A product are warming up to 40 ~ 50 DEG C, then by the polyoxyethylene glycol instillation flask after processed, reaction 2.5 ~ 3h, obtains B product;
C, B product are warming up to 75 ~ 80 DEG C, add Resorcinol, then by the Hydroxyethyl acrylate instillation after processed, reaction to-NCO group all disappears or content <0.5%, obtains finished product.
The preparation method of above-mentioned polyurethane acrylate prepolymer, the conciliation pH value described in step a, to 5, is, with composite organic acid, solution is reconciled PH to 5.
The preparation method of above-mentioned polyurethane acrylate prepolymer is by the polyoxyethylene glycol instillation flask after processed in step b by constant pressure funnel.
Paint prepared by aforesaid polyurethane acrylate prepolymer, comprises polyurethane acrylate prepolymer 50-60 part, two contracting propylene glycol double methacrylate 20-25 parts, ethoxylated trimethylolpropane triacrylate 5-15 part, 2-hydroxy-2-methyl-1-phenyl-1-acetone 3-10 part, 1-hydroxyl-ring ethyl benzophenone 1-5 part, polyacrylic ester 0.5-1 part, modified polyorganosiloxane 0.3-1 part, low molecule unsaturated carboxylic acid polymer 0.5-1 part, Resorcinol 0.1-0.5 part and hydrated magnesium silicate 2-6 part by mass parts.
Above-mentioned paint, comprises polyurethane acrylate prepolymer 54 parts, two contracting propylene glycol double methacrylates 22 parts, ethoxylated trimethylolpropane triacrylate 10 parts, 5 parts, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxyl-ring ethyl benzophenone 3 parts, polyacrylic ester 0.6 part, modified polyorganosiloxane 0.5 part, low molecule unsaturated carboxylic acid polymer 0.7 part, Resorcinol 0.2 part and hydrated magnesium silicate 4 parts by mass parts.
Beneficial effect of the present invention: compared with prior art, the present invention is optimized the formula of polyurethane acrylate prepolymer and preparation method, polyurethane acrylate prepolymer after obtained not only has superior toughness, flexibility, solidity to corrosion and adhesion strength, and can effectively retain original feature with the paint that this polyurethane acrylate prepolymer is obtained, be suitable as very much the raw material of Floor paint.In addition, applicant is also optimized by the preparation method of this polyurethane acrylate prepolymer preparation paint further, the paint prepared is made to have superior solidification rate high, and effectively can improve the glossiness on floor, snappiness and sticking power grade, result of use is very superior.After testing, all solidstate energy of paint that the present invention obtains reaches 450mj/cm 2solidification rate reaches 3s, the timber floor being simultaneously coated with this paint measures its glossiness by gloss of film degree (GB9754-1988) and reaches 50-70 °, its snappiness diameter < 1mm is measured by paint film flexibility (GB1731-1979), measuring sticking power grade by paint film adhesion grade (GB1720-1979) is 0, detected result shows, it is high that the timber floor being coated with this paint has glossiness, elasticity, snappiness are good, sticking power is good, the features such as impact resistance is good, and solidification rate is excellent.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but not as foundation the present invention being done to any restriction.
Embodiment 1: a kind of polyurethane acrylate prepolymer, this prepolymer comprises hexamethylene diisocyanate 1000 parts, dibutyl tin laurate 3 parts, polyoxyethylene glycol 500 parts, Resorcinol 2 parts and Hydroxyethyl acrylate 1150 parts by mass parts.
The preparation method of above-mentioned polyurethane acrylate prepolymer, comprises the following steps;
A, in the 500ml four-hole boiling flask that agitator, condenser, thermometer are housed, add the dibutyl tin laurate (DBTDL) of 3 parts of 1000 hexamethylene diisocyanates (HDI) and total charging capacity, pH value is reconciled to 5 with a small amount of composite organic acid, pass into dry nitrogen 5 ~ 10min, and stir with electric mixer, make it to be mixed to evenly, obtain A product;
B, A product are warming up to 40 ~ 50 DEG C, slowly instill in four-hole boiling flask in 1h with the polyoxyethylene glycol (PEG1000) 500 parts that the molecular-weight average after processed is 1000 by constant pressure funnel, reaction 2.5 ~ 3h, obtains B product;
C, B product are warming up to 75 ~ 80 DEG C, add Resorcinol 2 parts, then with dropping funnel, the Hydroxyethyl acrylate (HEA) 1150 parts after processed is instilled within the time of 1.5h, reaction 3h, extremely-NCO group all disappears or content <0.5%, obtained polyurethane acrylate prepolymer finished product.
Adopt paint prepared by above-mentioned polyurethane acrylate prepolymer, comprise polyurethane acrylate prepolymer 54 parts, two contracting propylene glycol double methacrylates 22 parts, ethoxylated trimethylolpropane triacrylate 10 parts, 5 parts, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxyl-ring ethyl benzophenone 3 parts, polyacrylic ester 0.6 part, modified polyorganosiloxane 0.5 part, low molecule unsaturated carboxylic acid polymer 0.7 part, Resorcinol 0.2 part and hydrated magnesium silicate 4 parts by mass parts.The preparation method of this paint can adopt conventional paint preparation method, polyurethane acrylate prepolymer by above-mentioned synthesis mixes according to the above ratio with raw materials such as two contracting propylene glycol double methacrylates, ethoxylated trimethylolpropane triacrylate, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxyl-ring ethyl benzophenone, polyacrylic ester, modified polyorganosiloxane, low molecule unsaturated carboxylic acid polymer, Resorcinol, hydrated magnesium silicates, be stirred to evenly, obtained paint.
Embodiment 2: a kind of polyurethane acrylate prepolymer, this prepolymer comprises hexamethylene diisocyanate 900 parts, dibutyl tin laurate 5 parts, polyoxyethylene glycol 500 parts, Resorcinol 2 parts and Hydroxyethyl acrylate 1300 parts by mass parts.
The preparation method of above-mentioned polyurethane acrylate prepolymer, comprises the following steps;
A, in the 500ml four-hole boiling flask that agitator, condenser, thermometer are housed, add the dibutyl tin laurate (DBTDL) of 3 parts of 1000 hexamethylene diisocyanates (HDI) and total charging capacity, pH value is reconciled to 5 with a small amount of composite organic acid, pass into dry nitrogen 5 ~ 10min, and stir with electric mixer, make it to be mixed to evenly, obtain A product;
B, A product are warming up to 40 ~ 50 DEG C, slowly instill in four-hole boiling flask in 1h with the polyoxyethylene glycol (PEG1000) 500 parts that the molecular-weight average after processed is 1000 by constant pressure funnel, reaction 2.5 ~ 3h, obtains B product;
C, B product are warming up to 75 ~ 80 DEG C, add Resorcinol 2 parts, then with dropping funnel, the Hydroxyethyl acrylate (HEA) 1150 parts after processed is instilled within the time of 1.5h, reaction 3h, extremely-NCO group all disappears or content <0.5%, obtained polyurethane acrylate prepolymer finished product.
Adopt paint prepared by above-mentioned polyurethane acrylate prepolymer, comprise polyurethane acrylate prepolymer 50 parts, two contracting propylene glycol double methacrylates 25 parts, ethoxylated trimethylolpropane triacrylate 15 parts, 7 parts, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxyl-ring ethyl benzophenone 3 parts, polyacrylic ester 0.6 part, modified polyorganosiloxane 0.5 part, low molecule unsaturated carboxylic acid polymer 0.7 part, Resorcinol 0.5 part and hydrated magnesium silicate 4 parts by mass parts.The preparation method of this paint can adopt conventional paint preparation method, polyurethane acrylate prepolymer by above-mentioned synthesis mixes according to the above ratio with raw materials such as two contracting propylene glycol double methacrylates, ethoxylated trimethylolpropane triacrylate, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxyl-ring ethyl benzophenone, polyacrylic ester, modified polyorganosiloxane, low molecule unsaturated carboxylic acid polymer, Resorcinol, hydrated magnesium silicates, be stirred to evenly, obtained paint.

Claims (5)

1. a polyurethane acrylate prepolymer, is characterized in that: this prepolymer comprises hexamethylene diisocyanate 1000 parts, dibutyl tin laurate 3 parts, polyoxyethylene glycol 500 parts, Resorcinol 2 parts and Hydroxyethyl acrylate 1150 parts by mass parts;
The preparation method of described polyurethane acrylate prepolymer, the method comprises the following steps;
A, hexamethylene diisocyanate to be mixed with dibutyl tin laurate, and adjust ph is to 5, then passes into dry nitrogen 5 ~ 10min, stir, obtain A product;
B, A product are warming up to 40 ~ 50 DEG C, then by the polyoxyethylene glycol instillation flask after processed, reaction 2.5 ~ 3h, obtains B product;
C, B product are warming up to 75 ~ 80 DEG C, add Resorcinol, then by the Hydroxyethyl acrylate instillation after processed, reaction to-NCO group all disappears or content <0.5%, obtains finished product.
2. polyurethane acrylate prepolymer according to claim 1, is characterized in that: the adjust ph described in step a, to 5, is, with composite organic acid, solution is regulated pH to 5.
3. polyurethane acrylate prepolymer according to claim 1, is characterized in that: be by the polyoxyethylene glycol instillation flask after processed in step b by constant pressure funnel.
4. the paint adopting the polyurethane acrylate prepolymer described in any one of claims 1 to 3 to prepare, is characterized in that: comprise polyurethane acrylate prepolymer 50-60 part, two contracting propylene glycol double methacrylate 20-25 parts, ethoxylated trimethylolpropane triacrylate 5-15 part, 2-hydroxy-2-methyl-1-phenyl-1-acetone 3-10 part, 1-hydroxyl-ring ethyl benzophenone 1-5 part, polyacrylic ester 0.5-1 part, modified polyorganosiloxane 0.3-1 part, low molecule unsaturated carboxylic acid polymer 0.5-1 part, Resorcinol 0.1-0.5 part and hydrated magnesium silicate 2-6 part by mass parts.
5. paint according to claim 4, is characterized in that: comprise polyurethane acrylate prepolymer 54 parts, two contracting propylene glycol double methacrylates 22 parts, ethoxylated trimethylolpropane triacrylate 10 parts, 5 parts, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxyl-ring ethyl benzophenone 3 parts, polyacrylic ester 0.6 part, modified polyorganosiloxane 0.5 part, low molecule unsaturated carboxylic acid polymer 0.7 part, Resorcinol 0.2 part and hydrated magnesium silicate 4 parts by mass parts.
CN201310004982.7A 2013-01-06 2013-01-06 Polyurethane acrylate prepolymer and preparation method thereof as well as paint prepared by same Active CN103030768B (en)

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CN103224604B (en) * 2013-04-23 2015-04-08 久盛地板有限公司 Modified epoxy acrylate and paint for wood underground heat floor prepared by the modified epoxy acrylate
CN109503808A (en) * 2018-10-31 2019-03-22 上纬新材料科技股份有限公司 Low viscous high-strength polyurethane acrylic resin of one kind and preparation method thereof
US11702384B2 (en) * 2019-12-06 2023-07-18 Skc Co., Ltd. Diisocyanate composition for optical lens and preparation method thereof
CN111072910A (en) * 2019-12-31 2020-04-28 湖南松井新材料股份有限公司 Nonionic polyurethane acrylate and preparation method and application thereof
CN114702852A (en) * 2022-04-24 2022-07-05 惠州市华士德化工有限公司 Slow-drying type ink diluent and preparation method thereof

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Denomination of invention: A kind of urethane acrylate prepolymer and preparation method thereof and paint prepared therewith

Effective date of registration: 20220803

Granted publication date: 20141217

Pledgee: Zhejiang Nanxun Rural Commercial Bank Co.,Ltd. Hengjie sub branch

Pledgor: JIUSHENG WOOD Co.,Ltd.

Registration number: Y2022330001614